2,2,2-Trifluoroethanol → 2-(2,2,2-Trifluoroethoxy)acetonitrile

Temperature

25 °C

At about 50° C., 26.4 g (0.40 mole) of 85% potassium hydroxide are solubilized in 100 g (1.0 mole) of 2,2,2-trifluoroethanol. After cooling at 25° C., 37.8 g (0.50 mole) of chloroacetonitrile are added dropwise to this solution. The temperature rises slowly to 40° C. and a precipitate appears. The reaction mixture is then brought gradually to 60° C.; after the addition of 300 ml of heptane, it is then brought to reflux. The whole of the vapour is condensed by means of a Dean and Stark apparatus. The lower phase of the condensate is separated after settling has taken place and distilled at atmospheric pressure. Yld: 19.6 g (28%), b.p. 125°-140° C.

1. customAt about 50° C.
2. customrises slowly to 40° C.
3. customis then brought gradually to 60° C.
4. temperatureto reflux
5. customcondensed by means of a Dean and Stark apparatus
6. customThe lower phase of the condensate is separated after settling
7. distillationdistilled at atmospheric pressure

ORD record

ord-b943d4f14e2f4df6a265ef01fb4d83dc

Source dataset

uspto-grants-1993_12

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US05270465